CN109111689B - Plastic composition for encapsulation and application thereof - Google Patents
Plastic composition for encapsulation and application thereof Download PDFInfo
- Publication number
- CN109111689B CN109111689B CN201710493178.8A CN201710493178A CN109111689B CN 109111689 B CN109111689 B CN 109111689B CN 201710493178 A CN201710493178 A CN 201710493178A CN 109111689 B CN109111689 B CN 109111689B
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- weight
- parts
- agent
- plastic composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
- C08G59/623—Aminophenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/04—Epoxynovolacs
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to the field of packaging materials, and discloses a plastic composition for packaging and application thereof. The plastic composition contains epoxy resin, a curing agent, silicon micropowder, an imidazole curing accelerator, a release agent, a silane coupling agent and a toughening agent in specific types and proportions, wherein the epoxy resin comprises liquid crystal epoxy resin, glycidylamine epoxy resin, o-cresol novolac epoxy resin and biphenyl epoxy resin, and the curing agent is melamine modified linear phenol-formaldehyde resin. The invention also discloses application of the composition in preparing plastic for packaging integrated circuits. The invention can obtain the packaging plastic with better performance by matching and using the specific epoxy resin, the curing agent, the filler, the auxiliary agent and the like, can be used for packaging large-scale integrated circuits, and is relatively green and environment-friendly.
Description
Technical Field
The invention relates to the field of packaging materials, in particular to a plastic composition for packaging and application thereof.
Background
With the progress of chip technology, the development of integrated circuits is moving towards high integration and surface mounting technology, and the development trend of electronic package and substrate materials adapted to the development is to make the materials have performance characteristics of low thermal expansion, high thermal conductivity, high heat resistance, and the like. Epoxy molding compound is one of the main raw materials for the subsequent packaging of Integrated Circuits (ICs), and its development is followed by the development of integrated circuits and packaging technology. Electronic products are developing towards high performance, multifunction, miniaturization and portability, and not only the performance requirements of integrated circuits are continuously improved, but also higher requirements are made on electronic packaging density. Epoxy molding compounds are also in constant demand for improvement and improvement. In order to meet the requirements of high-power discrete devices and high-heat devices, especially fully-encapsulated discrete devices on heat dissipation, high-thermal-conductivity fillers (such as CN106336620A) such as crystalline silica, alumina, aluminum nitride and boron nitride have been developed, and high-thermal-conductivity epoxy molding compounds are prepared by applying a high-filling technology, but the water absorption and heat resistance of the epoxy molding compounds do not meet ideal requirements.
In the two commands of WEEE and RoHS issued by the european union in 2003, six kinds of harmful materials, i.e., lead, hexavalent chromium, cadmium, polychlorinated biphenyl, halogenated flame retardants, radioactive substances, asbestos, etc., are prohibited from being used for a limited period of time in discarded electrical or electronic devices. Meanwhile, the information industry department of China also promulgates and implements 'pollution control and management methods for electronic information products', and the requirement of environmental protection for electronic products becomes an irreversible trend. In order to comply with two directive of European Union and national directive, the IC packaging material must be changed or improved to meet the environmental requirement. Therefore, there is a need to develop a halogen-free, antimony-free and phosphorus-free environment-friendly high-performance epoxy molding compound.
Disclosure of Invention
The invention aims to overcome the problems of poor performance (particularly water absorption and heat resistance) in the prior art and provide a plastic composition for packaging and application thereof.
In order to achieve the above object, one aspect of the present invention provides a plastic composition for encapsulation, comprising:
wherein the epoxy resin comprises liquid crystal epoxy resin, glycidylamine epoxy resin, o-cresol novolac epoxy resin and biphenyl epoxy resin, and the weight ratio of the liquid crystal epoxy resin to the glycidylamine epoxy resin to the o-cresol novolac epoxy resin to the biphenyl epoxy resin is (8-22) to (3-15) to (8-25) to (4.5-12.5); the curing agent is melamine modified linear phenolic resin.
The invention also provides the application of the plastic composition in preparing the plastic for packaging the integrated circuit.
The present invention provides, in a third aspect, a method for producing a plastic for encapsulation using the above plastic composition, the method comprising: the filler is subjected to surface treatment, melt mixing, cooling and crushing.
The invention can obtain the packaging plastic with high water absorption, high heat resistance, low viscosity, low expansion coefficient and high thermal conductivity under the condition of lower cost by using specific epoxy resin, curing agent, filler, auxiliary agent and the like in a matching way, and can be used for packaging large-scale integrated circuits. In addition, the invention can not use raw materials containing elements such as halogen, antimony, phosphorus and the like, can also meet the UL-94V-0 level flame retardant standard, and simultaneously can ensure the fluidity, operability and reliability of the plastic for packaging, thereby meeting the development requirement of environmental protection.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The present invention provides a plastic composition for encapsulation, which contains:
wherein the epoxy resin comprises liquid crystal epoxy resin, glycidylamine epoxy resin, o-cresol novolac epoxy resin and biphenyl epoxy resin, and the weight ratio of the liquid crystal epoxy resin to the glycidylamine epoxy resin to the o-cresol novolac epoxy resin to the biphenyl epoxy resin is (8-22) to (3-15) to (8-25) to (4.5-12.5); the curing agent is melamine modified linear phenolic resin.
According to the present invention, the epoxy resin includes at least the above four epoxy resins. In a preferred embodiment of the present invention, the content of the epoxy resin is 30 to 47 parts by weight. In a further preferred embodiment, the epoxy resin is present in an amount of 16.9 to 34.3 parts by weight per 100 parts by weight of filler.
In the present invention, the liquid crystal epoxy resin (a liquid crystal epoxy resin other than a biphenyl type epoxy resin) is particularly useful for improving melt viscosity, processability, thermal expansion coefficient, water absorption, moisture resistance, glass transition temperature, dip and reflow resistance, toughness and reducing fine silica powder content. In a more preferred embodiment of the present invention, the content of the liquid crystal epoxy resin is 6.1 to 8.9 parts by weight with respect to 100 parts by weight of the filler. The liquid crystal epoxy resin can be aromatic ester, biphenyl, alpha-methyl styrene and methylene amine, can be in a main chain type or a side chain type, but is a thermotropic liquid crystal, and the liquid crystal phase transition temperature is usually within 95-150 ℃. Preferably, the liquid crystal epoxy resin is JEC-832 of Jiangshan Jiangxi Huanju chemical industries, Ltd, or HP-4032D of Japanese DIC Corporation.
In the present invention, the glycidylamine-type epoxy resin is particularly advantageous in improving aging resistance, acid resistance and reducing water absorption. In a more preferred embodiment of the present invention, the glycidyl amine type epoxy resin is contained in an amount of 1.7 to 10 parts by weight with respect to 100 parts by weight of the filler. The glycidyl amine type epoxy resin may be conventionally selected in the art, and for example, may be at least one of diaminodiphenylmethane tetraglycidyl amine, diglycidyl p-aminophenol, triglycidyl-p-aminophenol (TGPAP), and N, N '-tetraglycidyl-4, 4' -diaminodiphenylmethane (TGDDM), etc. The basic structure of the glycidylamine-type epoxy resin is preferably as shown by the following formula:
in the invention, the o-cresol formaldehyde epoxy resin is particularly beneficial to increasing the crosslinking density, improving the heat resistance of the composition and reducing the cost. In a more preferred embodiment of the present invention, the o-cresol novolac epoxy resin is contained in an amount of 6.1 to 9.5 parts by weight, relative to 100 parts by weight of the filler. The O-cresol formaldehyde epoxy resin can be selected conventionally and is generally obtained by reacting O-cresol formaldehyde resin (O-CN) and Epichlorohydrin (ECH), and the basic structure of the O-cresol formaldehyde epoxy resin can be shown as formula I:
in formula I, m is preferably any integer between 10 and 100. The o-cresol novolac epoxy resin used in the present invention may be commercially available, such as N-665 available from DIC Corporation of Japan.
In the present invention, the biphenyl type epoxy resin is particularly advantageous for heat resistance and water resistance of the plastic for encapsulation. In a more preferred embodiment of the present invention, the biphenyl type epoxy resin is contained in an amount of 3 to 5.9 parts by weight, relative to 100 parts by weight of the filler. The biphenyl type epoxy resin can be selected conventionally, and the basic structure of the biphenyl type epoxy resin can be shown as a formula II:
in formula II, k is preferably any integer between 10 and 100. The biphenyl type epoxy resin used in the present invention can be obtained commercially, for example, JPPN-603 of Jiangshan Jiangxi chemical industries, Ltd, BRG-557 of Showa polymer, NC-3000 series of Japan Chemicals, Minghe H-1.
In a further preferred embodiment, the weight ratio between the liquid crystal epoxy resin, the glycidylamine type epoxy resin, the o-cresol novolac epoxy resin and the biphenyl type epoxy resin is 1 (0.2-1.3): (1-1.1): (0.5-0.7). The use of the plastic composition of the preferred embodiment to prepare a plastic for encapsulation can further improve the properties of the resulting plastic for encapsulation.
According to the invention, the curing agent (or the melamine modified linear phenolic resin) has excellent curing performance on the epoxy resin, and is particularly beneficial to improving the crosslinking density, thereby improving the heat resistance of the plastic for encapsulation. The curing agent is beneficial to increasing the thermal deformation temperature of the plastic for encapsulation (which can be increased to 260 ℃ to 290 ℃). In a preferred embodiment of the present invention, the curing agent is contained in an amount of 15 to 22 parts by weight. In a further preferred embodiment, the curing agent is present in an amount of 11.5 to 13.4 parts by weight per 100 parts by weight of filler. The melamine modified phenol novolac resin is obtained by modifying phenol novolac resin with melamine, which can be selected conventionally, the basic structure is generally shown as formula III, and the (unmodified) phenol novolac resin is generally prepared from formaldehyde and phenol (benzene ring is substituted or unsubstituted) by (0.75-0.85): 1 to give:
in formula III, n is preferably an integer from 1 to 50, and o is preferably an integer from 1 to 50.
According to the invention, the silicon micropowder is particularly beneficial to improving the filling amount, increasing the thermal conductivity of the plastic for packaging and reducing the linear expansion coefficient. In a preferred embodiment of the present invention, the content of the fine silica powder is 130-170 parts by weight. The silica powder can be silica powder commonly used in the field, and preferably, the silica powder is fused spherical silica powder. Wherein the particle diameter of the fused spherical silicon micropowder can be 0.1-30 μm, the spheroidization rate is more than 95%, the conductivity is less than or equal to 1 μ s/cm, the sodium ion content is less than or equal to 1ppm, the chloride ion content is less than or equal to 3ppm, and the specific surface area<40m2G, glass transition rate (degree of non-crystallinity)>97％。
According to the invention, the plastic composition may also contain a stress-relieving agent which facilitates the release of the internal stress of the molding compound. In a preferred embodiment of the present invention, the stress releasing agent is contained in an amount of 0.3 to 5 parts by weight. In a further preferred embodiment, the stress release agent is present in an amount of 0.2 to 3.4 parts by weight, relative to 100 parts by weight of filler. The stress releasing agent may be conventionally selected, but preferably, the stress releasing agent is at least one of silicone oil, acrylonitrile butadiene, rubber, and polybutylene acrylate.
According to a preferred embodiment of the present invention, the imidazole-based curing accelerator is contained in an amount of 0.4 to 0.8 parts by weight. In a further preferred embodiment, the imidazole-based curing accelerator is present in an amount of 0.2 to 0.5 parts by weight per 100 parts by weight of filler. The imidazole-based curing accelerator may be various imidazole-based materials commonly used in the art, and preferably, the imidazole-based curing accelerator is at least one of 2-methylimidazole (2MZ), 1-cyanoethyl-2-methylimidazole (2MZCN) and 2-ethyl-4-methylimidazole (2E4 MZ).
According to a preferred embodiment of the present invention, the content of the release agent is 2.5 to 3 parts by weight. In a further preferred embodiment, the content of the release agent is 1.6 to 2.2 parts by weight relative to 100 parts by weight of the filler. The release agent may be one commonly used in the art, but is preferably stearic acid and/or a stearate salt. The stearate may be sodium stearate and/or potassium stearate.
According to a preferred embodiment of the present invention, the silane coupling agent is contained in an amount of 1.5 to 2 parts by weight. In a further preferred embodiment, the content of the silane coupling agent is 1 to 1.4 parts by weight with respect to 100 parts by weight of the filler. The silane coupling agent may be conventionally selected in the art, and for example, may be at least one of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-mercaptopropyltriethoxysilane, gamma-mercaptopropyldimethoxysilane, and azidosilane.
According to the invention, the use of the toughening agent is particularly beneficial to improving the impact toughness of the packaging plastic, thereby improving the thermal stress cracking resistance and avoiding stress cracking in the high-temperature dip soldering and reflow soldering processes. According to a preferred embodiment of the present invention, the content of the toughening agent is 5 to 6 parts by weight. In a further preferred embodiment, the content of the toughening agent is 2.9 to 4.7 parts by weight with respect to 100 parts by weight of the filler. The toughening agent may be a toughening agent commonly found in the art, but in a preferred embodiment, the toughening agent is at least one of a carboxyl-terminated liquid nitrile rubber, a hydroxyl-terminated liquid polybutadiene, and a liquid silicone rubber. The liquid silicone rubber is not only beneficial to improving the impact toughness of the plastic for packaging, but also contributes to flame retardance.
The invention can effectively improve the performance of the plastic for packaging under the condition of not using raw materials containing elements such as halogen, antimony, phosphorus and the like. Therefore, in order to meet the development requirements of green environmental protection, in a preferred embodiment of the present invention, the total content of halogen, antimony, phosphorus and metal oxide in the plastic composition is below 0.001 wt%, and more preferably, the plastic composition is free of halogen, antimony, phosphorus and metal oxide.
According to the invention, the plastic composition may also contain colorants in order to impart a certain color to the plastic. The content of the colorant may be 3 to 6 parts by weight. In a more preferred embodiment, the colorant is present in an amount of 1.7 to 2.4 parts by weight per 100 parts by weight of filler. The colorant may be a colorant conventionally used in the art, and preferably, the colorant is at least one of carbon black, chrome blue, chrome green, chrome yellow, and molybdate.
It is to be specifically noted that, although the main functions of the respective components in the plastic composition of the present invention are described above separately, it is not intended to indicate that they exert only the above-mentioned functions in the plastic composition, but on the contrary, in the plastic composition of the present invention, the respective components supplement each other and act synergistically as an organic whole to achieve the above-mentioned object. According to a preferred embodiment of the invention, the plastic composition consists only of the above-mentioned ingredients. The resins used in the present invention are all commercially available, and may be obtained from commercially available sources as described in examples.
The invention also provides application of the plastic composition in preparing plastic for packaging integrated circuits.
In addition, the invention provides a method for preparing plastic for encapsulation by using the plastic composition, which comprises the following steps: the filler is subjected to surface treatment, melt mixing, cooling and crushing.
In order to further improve the performance of the plastic for packaging, in a preferred embodiment of the invention, the method further comprises removing metal impurities from the raw material and/or the crushed material by a magnetic separation method. More specifically, the magnetic separation may be performed after the surface treatment, to remove the metal impurities by performing the magnetic separation on each component, or may be performed after the pulverization to further remove the metal impurities by performing the magnetic separation on the material. The magnetic separation can be carried out by a sieve with magnetism (the aperture of the sieve is 1-2mm), and the metal impurities are adsorbed by the sieve and are left on the sieve, so that the metal impurities are conveniently removed.
In practice, the method may comprise: after the components are accurately weighed, the filler is treated by the silane coupling agent in a mixer, the mixture is firstly mixed for 3 to 5 minutes and then kept stand for 3 to 7 minutes, and the surface treatment is carried out by repeating the steps for many times; then adding other components in proportion, detecting by using a metal detector, removing metal impurities through magnetic separation, mixing for 3-5 minutes, melting and mixing the mixture, wherein the mixing temperature can be 95-135 ℃, and the mixing time can be 3-5 minutes; and cooling the product, crushing, sieving, conveying by a pipeline, carrying out magnetic separation, stirring, mixing and tabletting.
The present invention will be described in detail below by way of examples.
In the following examples, the sources of the individual components are as follows:
polyfunctional epoxy resin: TGDDM, JEPN-838, Jiangshan Jianghua chemical industries, Inc.;
liquid crystal epoxy resin: JEC-832, Jiangshan Jiangxi chemical industries, Ltd;
o-cresol novolac epoxy resin: JECN-804, Jiangshan Jiangxi chemical industries, Ltd;
biphenyl type epoxy resin: JPPN-603, Jiangshan Jianghua chemical industries, Ltd;
modified phenolic resin: JECN-803S, Jiangshan Jiangxi chemical industries, Ltd;
colorant: carbon black, Beijing reagent company;
stearic acid (mold release agent): chemically pure, Beijing reagent company;
imidazole curing accelerator: 2MZ (example 1) or 2MZCN (examples 2 and 3), Guangzhou Chuanjing electronics materials, Inc.;
silicon micropowder: QG75, yunnan research institute for nonmetallic minerals;
a toughening agent: carboxyl-terminated liquid nitrile rubber, A-658, Shenzhen Jinda Total science and technology, Inc.;
silane coupling agent: gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, KH-560, Wuhan Silicone New materials, Inc.
Example 1
The method for preparing the plastic for packaging comprises the following steps: accurately weighing the components (g) as shown in Table 1, treating the filler with a silane coupling agent in a mixer, mixing for 5 minutes, standing for 3 minutes, and repeating the above steps for 5 times to perform surface treatment; then adding other components in proportion, detecting by using a metal detector, removing metal impurities through magnetic separation, mixing for 3 minutes, melting and mixing the mixture, wherein the mixing temperature is 100 ℃, and the mixing time is 4 minutes; and cooling the product, crushing and sieving (taking undersize materials of a 100-mesh sieve), carrying out pipeline transmission, carrying out magnetic separation, stirring and mixing, tabletting and carrying out performance test. The performance test method comprises the following steps:
detecting the heat conductivity with a heat conductivity tester (Andry 3001-II, Technological development of Tianjin Yinbel Co., Ltd.);
melt viscosity: measured using a high flow meter from Shimadzu corporation, Japan, test conditions: the mouth mold is 0.5 multiplied by 1mm, the load is 10kg, and the temperature is 175 ℃;
water absorption: the sample was dried at 120 ℃ for 4 hours, and 20g of the dried sample was weighed as a sample (denoted by w)1) The sample to be tested is soaked in 50g of deionized water for 30 minutes, after filtration, the solid phase is drained for 5 minutes, and the weight of the drained solid phase is then weighed (denoted as w)2) The water absorption was calculated using the following formula:
glass transition temperature (Tg): the glass transition temperature of the composition was measured using a thermomechanical analyzer (TA, TMA, USA), and a sample of the molding material was formed into a block having a diameter of 3mm and a height of 6mm at 175 ℃/25MPa, and then cured at 175 ℃/6h, and then tested by the TMA test under the following conditions: the temperature is 20-300 ℃, and the heating rate is 10 ℃/min;
the thermal expansion coefficients (α 1, α 2) were measured by a thermomechanical analyzer (TMA): using a thermomechanical analyzer (TMA100, セイコー, manufactured by electronics industries, Ltd.), a load of 50mN was applied, and the temperature was measured at a rate of 10 ℃/min to obtain an average value of 100-;
the bending strength and the bending elastic modulus are tested by using a universal testing machine;
flame retardancy: flame resistance tests were carried out by the vertical combustion method in accordance with GB 4609-84.
The results of the performance tests are also shown in table 1.
Comparative example 1
Plastics for encapsulation were prepared according to the method of example 1, but the contents of the liquid crystal epoxy resin, the o-cresol novolac epoxy resin, the modified phenol resin and the biphenyl-containing epoxy resin were different (see table 1), and the results of the performance test are also shown in table 1.
Comparative example 2
Encapsulation plastics were prepared according to the method of example 1, but with different levels of imidazole-based curing accelerators, silane coupling agents and toughening agents (see table 1), and the results of the performance tests are also shown in table 1.
Comparative example 3
A plastic for encapsulation was prepared in accordance with the procedure of example 1, except that the o-cresol novolac epoxy resin was replaced with "dicyclopentadiene phenol type epoxy resin (HP-7200H, available from DIC Corporation of Japan)", and the results of the performance tests were also shown in Table 1.
Comparative example 4
Encapsulation plastic was prepared according to the method of example 1, except that the multifunctional epoxy resin was replaced with a liquid crystal epoxy resin, and the performance test results are also shown in table 1.
TABLE 1
As can be seen from the results in Table 1, the plastic composition of the present invention can be used to prepare packaging plastics with high water absorption, high heat resistance, low viscosity, low expansion coefficient and high thermal conductivity, and is free of halogen, antimony, phosphorus and other elements, and environmentally friendly. Further, as can be seen by comparing example 1 with comparative examples 1 to 4, respectively, the above properties (particularly water absorption and heat resistance) can be effectively improved only by compounding specific kinds and amounts of epoxy resin, curing agent, filler, auxiliary agent and the like.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (8)
1. A plastic composition for encapsulation, characterized in that the plastic composition comprises:
30-47 parts by weight of epoxy resin,
15-22 parts by weight of a curing agent,
130 portions of silicon micro powder and 170 portions of silicon micro powder,
0.4 to 0.8 weight portion of imidazole curing accelerator,
2.5 to 3 weight portions of release agent,
1.5 to 2 weight portions of silane coupling agent,
5-6 parts of a toughening agent,
wherein the epoxy resin comprises liquid crystal epoxy resin, glycidylamine epoxy resin, o-cresol formaldehyde epoxy resin and biphenyl epoxy resin, and the weight ratio of the liquid crystal epoxy resin to the glycidylamine epoxy resin to the o-cresol formaldehyde epoxy resin to the biphenyl epoxy resin is 1 (0.2-1.3) to 1-1.1 to 0.5-0.7; the curing agent is melamine modified linear phenolic resin.
2. The plastic composition according to claim 1, wherein the content of the liquid crystal epoxy resin is 6.1 to 8.9 parts by weight, the content of the glycidylamine-type epoxy resin is 1.7 to 10 parts by weight, the content of the o-cresol novolac epoxy resin is 6.1 to 9.5 parts by weight, the content of the biphenyl-type epoxy resin is 3 to 5.9 parts by weight, the content of the curing agent is 11.5 to 13.4 parts by weight, the content of the imidazole-type curing accelerator is 0.2 to 0.5 part by weight, the content of the release agent is 1.6 to 2.2 parts by weight, the content of the silane coupling agent is 1 to 1.4 parts by weight, and the content of the toughening agent is 2.9 to 4.7 parts by weight, relative to 100 parts by weight of the filler.
3. The plastic composition of claim 1, wherein the micropowder of silica is a fused spherical micropowder of silica;
and/or the imidazole curing accelerator is at least one of 2-methylimidazole, 1-cyanoethyl-2-methylimidazole and 2-ethyl-4-methylimidazole;
and/or the release agent is stearic acid and/or stearate;
and/or the silane coupling agent is at least one of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-aminopropyl triethoxy silane, gamma-mercaptopropyl dimethoxy silane and azido silane;
and/or the toughening agent is at least one of carboxyl-terminated liquid nitrile rubber, hydroxyl-terminated liquid polybutadiene and liquid silicone rubber.
4. The plastic composition of claim 1, wherein the plastic composition further comprises 3 to 6 parts by weight of a colorant.
5. The plastic composition of claim 4, wherein the colorant is at least one of carbon black, chrome blue, chrome green, chrome yellow, and molybdate.
6. Use of the plastic composition according to any one of claims 1 to 5 for the preparation of a plastic for the encapsulation of integrated circuits.
7. A method for preparing a plastic material for encapsulation using the plastic composition of any one of claims 1 to 5, comprising: the filler is subjected to surface treatment, melt mixing, cooling and crushing.
8. The method of claim 7, further comprising removing metal impurities from the feedstock and/or the pulverized material using a magnetic separation process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710493178.8A CN109111689B (en) | 2017-06-26 | 2017-06-26 | Plastic composition for encapsulation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710493178.8A CN109111689B (en) | 2017-06-26 | 2017-06-26 | Plastic composition for encapsulation and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109111689A CN109111689A (en) | 2019-01-01 |
| CN109111689B true CN109111689B (en) | 2020-11-24 |
Family
ID=64733803
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710493178.8A Expired - Fee Related CN109111689B (en) | 2017-06-26 | 2017-06-26 | Plastic composition for encapsulation and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109111689B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113969125A (en) * | 2021-09-24 | 2022-01-25 | 法拉新材料(连云港)有限公司 | High-adhesion anti-cracking epoxy powder composition and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029165A (en) * | 2006-03-01 | 2007-09-05 | 广东榕泰实业股份有限公司 | Epoxy-resin mould plastic for packing IC circuit and its production |
| CN102030968A (en) * | 2009-09-30 | 2011-04-27 | 北京科化新材料科技有限公司 | Epoxy resin composition for encapsulating semiconductor device and preparation method thereof |
| CN104927310A (en) * | 2014-03-17 | 2015-09-23 | 中国石油化工股份有限公司 | Epoxy resin composition and epoxy resin material obtained by curing |
| CN106674910A (en) * | 2016-12-22 | 2017-05-17 | 科化新材料泰州有限公司 | Low-stress epoxy plastic packaging material for semiconductor packaging |
-
2017
- 2017-06-26 CN CN201710493178.8A patent/CN109111689B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029165A (en) * | 2006-03-01 | 2007-09-05 | 广东榕泰实业股份有限公司 | Epoxy-resin mould plastic for packing IC circuit and its production |
| CN102030968A (en) * | 2009-09-30 | 2011-04-27 | 北京科化新材料科技有限公司 | Epoxy resin composition for encapsulating semiconductor device and preparation method thereof |
| CN104927310A (en) * | 2014-03-17 | 2015-09-23 | 中国石油化工股份有限公司 | Epoxy resin composition and epoxy resin material obtained by curing |
| CN106674910A (en) * | 2016-12-22 | 2017-05-17 | 科化新材料泰州有限公司 | Low-stress epoxy plastic packaging material for semiconductor packaging |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109111689A (en) | 2019-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113201204B (en) | High Tg and low warp MUF epoxy resin composition and preparation method thereof | |
| JP2007246861A (en) | Resin composition, and varnish obtained using the resin composition, film adhesive, and copper foil attached with film adhesive | |
| CN109111689B (en) | Plastic composition for encapsulation and application thereof | |
| KR930003800B1 (en) | Semiconductor encapsulant consisting of epoxy resin composition | |
| CN109111685B (en) | Plastic composition for encapsulation and application thereof | |
| JP3309661B2 (en) | Epoxy resin composition and semiconductor device | |
| CN109111688B (en) | Plastic composition for encapsulation and application thereof | |
| CN109111687B (en) | Plastic composition for encapsulation and application thereof | |
| CN109111686B (en) | Plastic composition for encapsulation and application thereof | |
| JP2001261939A (en) | Liquid resin composition and semiconductor device by using the same | |
| KR101279973B1 (en) | Epoxy resin composition for encapsulating semiconductor element and semiconductor element package using the same | |
| KR101437141B1 (en) | Epoxy resin composition for encapsulating semiconductor | |
| KR100529258B1 (en) | Epoxy Molding Compound for Excapsulation of Semiconductor | |
| KR100440599B1 (en) | Resin composition comprising semi-spherical silica for sealing semiconductor devices and preparation method thereof | |
| KR20110078440A (en) | Non-solvent type surface treatment agent, inorganic particles surface-treated with the agent, epoxy resin composition for encapsulating semiconductor device includding the particles and semiconductor apparatus using the composition | |
| JP2005290111A (en) | Resin composition for encapsulation and semiconductor device | |
| JPH07107091B2 (en) | Epoxy resin composition for semiconductor encapsulation | |
| KR20100072720A (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device using the same | |
| JP2005281624A (en) | Resin composition for sealing and semiconductor device | |
| CN114685935B (en) | Low dielectric constant resin composition and preparation method and application thereof | |
| KR102319561B1 (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same | |
| KR100882541B1 (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device using the same | |
| KR101234846B1 (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device using the same | |
| KR100882336B1 (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device using the same | |
| KR101234843B1 (en) | Epoxy resin composition for encapsulating semiconductor device and semiconductor device using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20201124 Termination date: 20210626 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |